EP1215310A1 - P-typ zinkoxid-einkristall mit niedrigem widerstand und herstellungsverfahren dafür - Google Patents

P-typ zinkoxid-einkristall mit niedrigem widerstand und herstellungsverfahren dafür Download PDF

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Publication number
EP1215310A1
EP1215310A1 EP00942475A EP00942475A EP1215310A1 EP 1215310 A1 EP1215310 A1 EP 1215310A1 EP 00942475 A EP00942475 A EP 00942475A EP 00942475 A EP00942475 A EP 00942475A EP 1215310 A1 EP1215310 A1 EP 1215310A1
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type
zinc oxide
crystal
resistivity
low
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French (fr)
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EP1215310B1 (de
EP1215310A4 (de
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Tetsuya B-102 Saison Meruveille haruto YAMAMOTO
Hiroshi Yoshida
Takafumi Yao
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Japan Science and Technology Agency
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Japan Science and Technology Agency
Japan Science and Technology Corp
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
    • C30B23/02—Epitaxial-layer growth
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/16—Oxides

Definitions

  • the present invention relates to a low-resistivity p-type single-crystal zinc oxide (ZnO) and a method of preparing the same.
  • n-type ZnO low-resistivity n-type ZnO by a conventional B, Al, Ga or In doping technique without any difficulty.
  • p-type ZnO there have been only reports on a high-resistivity p-type ZnO obtained by N (Nitrogen) doping.
  • N (Nitrogen) doping one N-doped p-type ZnO was reported from Kasuga Laboratory of Engineering Department of Yamanashi University in the 59th Meeting of the Japan Society of Applied Physics (Lecture No. 17p-YM-8, Japanese Journal of Applied Physics, Part 2, vol. 36, No. 11A, p. 1453, 1 Nov. 1997).
  • the p-type ZnO thin film prepared by Kasuga Laboratory of Engineering Department of Yamanashi University is not suitable for practical use because of still high resistivity of 100 ⁇ ⁇ cm. Further, the p-type ZnO thin film has a remaining problem of experimental repeatability in that its conduction type is inversely changed from p-type to n-type after annealing, and has not been developed to an effective low-resistivity p-type ZnO.
  • Li is one element of the first group of the Periodic System and is assumed as an acceptor for fabricating p-type materials.
  • Li-doping has been used only for fabricating high-resistivity ZnO thin films, and such doping effects are being studied in a field of dielectric materials as electrical insulators rather than materials for semiconductor devices.
  • Akira Onodera (Graduate School of Science, Hokkaido University) has reported to prepare a Li-doped ZnO having a high resistivity (specific resistance) of 10 10 ⁇ ⁇ cm as a memory material by one crystal growth method, so-called hydrothermal method.
  • a p-type ZnO having a low resistivity can be synthesized as a ZnO single-crystal thin film, it becomes possible to achieve a p-n junction between ZnO (zinc oxide) semiconducting compounds of the same kind by combining the synthesized low-resistivity p-type ZnO with the low-resistivity n-type ZnO (zinc oxide) which has already been put into practice through the impurity doping process using 8 (Boron), Al (Aluminum), Ga (Gallium) or In (Indium).
  • This p-n junction makes it possible to fabricate various semiconductor devices, such as an implantation type light-emitting diode, laser diode and thin film solar cell, with high quality and low cost.
  • various semiconductor devices such as an implantation type light-emitting diode, laser diode and thin film solar cell, with high quality and low cost.
  • the above ZnO can be used for fabricating an ultraviolet laser diode necessary for high-density recording or large-scale information transfer.
  • the inventors have developed a novel doping method for incorporating a p-type dopant into ZnO to achieve enhanced stabilization in ZnO.
  • the present invention is directed to a low-resistivity p-type single-crystal ZnO containing a p-type and an n-type.
  • the present invention is also directed to a low-resistivity p-type single-crystal ZnO containing a p-type, an n-type, and the second group element.
  • the n-type dopant may be one or more elements selected from the group consisting of B, Al, Ga, In, Zn, F, Cl and H.
  • the p-type element may be one or more elements selected from the group consisting of the first group elements, the fifth group elements and C, preferably of Li, Na, N and C.
  • the concentration ratio of the contained p-type dopant to the contained n-type dopant is preferably set in the range of 1.3 : 1 to 3 : 1, most preferably in 2 : 1.
  • the low-resistivity p-type single-crystal ZnO according to the present invention has a hole concentration of 2 x 10 18 /cm 3 or more, more preferably 1 x 10 19 /cm 3 or more. Further, the low-resistivity p-type single-crystal ZnO has an electrical resistivity of 20 ⁇ ⁇ cm or less, more preferably 10 ⁇ ⁇ cm or less, more specifically less than 1 ⁇ ⁇ cm.
  • the n-type dopant and p-type dopant are pared up in a ZnO single-crystal by doping the n-type and p-type dopants into the ZnO single crystal.
  • carriers will be scattered not by the p-type dopants with a charge but by p-type dopants with a smaller charge, to be screened by virtue of the n-type dopant having an opposite charge to that of the p-type dopant.
  • the hole mobility of carriers is significantly increased, and thereby a desired low-resistivity p-type single-crystal ZnO can be obtained.
  • the second group elements of the Periodic System have no influence on the conduction type, and contribute to stabilization of oxygens in the basal ZnO semiconducting compound to carry out a function of reducing the concentration of oxygen vacancy.
  • Mg and/or Be are particularly desirable to achieve this function.
  • the present invention is directed to a method of preparing a low-resistivity p-type single-crystal zinc oxide in which an n-type dopant and p-type dopant are doped into zinc oxide with higher concentration of the p-type dopant than that of the n-type dopant during forming a single-crystal of the zinc oxide through a thin film forming process.
  • the present invention is directed to a method of preparing a low-resistivity p-type single-crystal zinc oxide in which n-type and p-type dopants and at least one of Mg and Be are doped into zinc oxide with higher concentration of the p-type dopant than that of the n-type dopant and that of the at least one of Mg and Be during forming a single-crystal of the zinc oxide through a thin film forming process.
  • the thin film forming process may include the step of supplying an atomic gas from a Zn solid source and an active oxygen onto a semiconductor substrate to grow a single-crystal zinc oxide thin film on the substrate.
  • an atomic gas vaporized from a Zn solid source by use of MOCVD (Metal Organic Chemical Vapor Deposition) or MBE (Molecular Beam Epitaxy) using an atomic beam and an active oxygen may be flowingly supplied onto and deposited at a low temperature on a semiconductor substrate to grow a single-crystal zinc oxide thin film on the semiconductor substrate under sufficient oxygen plasma.
  • MOCVD Metal Organic Chemical Vapor Deposition
  • MBE Molecular Beam Epitaxy
  • the doped p-type and n-type dopants can suppress the increase of electrostatic energy due to Coulomb's reaction force between the p-type dopants, and can bring out Coulomb's attraction force between the n-type and p-type dopants to create an energy gain.
  • the gain from the above electrostatic interaction allows more p-type dopants to be effectively incorporated, so as to achieve further enhanced stabilization of the ionic charge distributions in ZnO.
  • the p-type dopant can be stably doped in a high concentration. While the n-type and p-type dopants may be doped separately at different timings, it is desired to simultaneously dope or co-dope them.
  • the higher concentration of the p-type dopant than that of the n-type dopant can be specifically provided by adjusting their amount to be incorporated or the pressure of the atomic gas.
  • the p-type dopant and/or the n-type dopant and/or the second group element can be transformed into an atomic form by electronically exciting them with the use of radiofrequency waves, lasers, X-rays or electron beams.
  • the substrate has a temperature ranging from 300°C to 650°C.
  • the temperature less than 300°C causes extremely reduced growth rate of the thin film, which is not suitable for practical use.
  • the temperature higher than 650°C causes intensive oxygen escaping, resulting in increased defects, degraded crystallization and lowered doping effects.
  • the substrate may include a silicon single-crystal substrate, a silicon single-crystal substrate having a SiC layer formed therein and a sapphire single-crystal substrate.
  • the substrate has the same crystal structure as that of ZnO, and has almost the same lattice constant as that of ZnO.
  • the substrate and thin film may interpose therebetween a chromium oxide layer or titanium oxide layer having an average valve of respective lattice constants of the substrate and thin film to reduce unconformity in crystal lattices.
  • the formed single-crystal zinc oxide is cooled down to room temperature, and then subjected to a heat treatment at a high temperature ranging, for example, from about 100 to 250°C under an electric field. This allows hydrogen, which in generally behave as a donor, to be removed outside.
  • the size of energy gap can be freely controlled by combining the low-resistivity p-type single-crystal ZnO with the conventional low-resistivity n-type ZnO (zinc oxide).
  • This provides an optoelectronics material having a high performance over the range from visible light to ultraviolet light and a wide range of application in an implantation type light-emitting diode or laser diode. Further, the applicable area can be expanded to various photoelectric conversion devices or low-resistivity semiconductors such as a solar cell.
  • a magnetism-semiconductor hybrid-function element can be fabricated by doping a transition metal, Mn, Fe or Co, which is a magnetic element, into the thin layer of the low-resistivity p-type single-crystal ZnO.
  • a donor-acceptor pair e.g. Li-F-Li or N-Ga-N
  • a donor-acceptor pair is formed in the crystal, (1) to suppress the increase of electrostatic energy due to Coulomb's reaction force between the p-type dopants, and increase the solubility of additional p-type dopants, and (2) to allow the scattering extent of the dopants acting to the dynamics of holes, which is 100 angstroms or more in a single doping, to interact in a shorter range of several tens of angstroms, and thus allows average free mobility of carriers to be increased.
  • the second group element is doped (3) to form a strong chemical bonding between Mg-O or Be-O in the crystal so as to prevent oxygen escaping.
  • the above three effects make it possible to dope the p-type dopant stably in a high concentration, and the resulting low-resistivity p-type single-crystal ZnO can be used as an optoelectronics material over the range from visible light to ultraviolet light
  • the single crystal ZnO thin film is particularly subject to oxygen escaping
  • one or more elements selected from the group consisting of B, Al, Ga, In, Zn, F, Cl and H occupy the resulting oxygen vacancy to prevent the degradation of crystallization due to the vacancy formation
  • the p-type dopant typically one or more elements selected from the group consisting of Li, Na, N and C, is stabilized at Zn coordination (O coordination in case of N) by ionic bonding.
  • F F
  • Li 1 : 2.
  • a strong chemical bonding is created between the adjacent F and Li to form a complex of Li-F-Li in the ZnO crystal thin film.
  • the energy in lattice system is increased, and thereby an oxygen vacancy is induced.
  • the vacancy acts as a donor and causes the degradation of crystallization.
  • the Li moves between lattices, and thereby the roll of the Li is inversely changed from acceptor to donor. This blocks the creation of a low-resistivity p-type single-crystal ZnO thin film.
  • the doped Li is stabilized after the complex is formed and thereby the stabilized Li moves to shallow level. This allows more carriers to be created at lower temperature (at the temperature closer to room temperature) to provide a desired low-resistivity p-type single-crystal ZnO thin film.
  • a sapphire substrate 2 was placed in a vacuum chamber 1 having a maintained internal pressure of 10 -8 Torr, and an atomic Zn gas and an atomic O gas were supplied onto the substrate 2 to fablicate a ZnO thin film on the substrate 2.
  • the atomic Zn gas was prepared by heating a Zn solid source having a purity of 99,99999% with a heater to bring it into an atomic form.
  • the atomic O gas was prepared by activating oxygen having a purity of 99.99999% with an RF radical cell.
  • Each of Li serving as a p-type acceptor and F serving as an n-type donor was prepared by radiating the microwave level of electromagnetic waves to a corresponding molecular gas or by bringing a corresponding elemental cell into an atomic form under a high temperature.
  • Fig. 1 shows an RF (radio frequencies) coil 3, a heater 4, and an elemental cell (Li source) 5, which are used in this method.
  • F as an n-type dopant and Li as a p-type dopant were simultaneously supplied onto the substrate 2 at a partial pressures of 10 -7 Torr and a partial pressure of 5x10 -7 Torr, respectively, to induce the crystal growth for forming a p-type single-crystal ZnO thin film 6 at each temperature of 350°C, 400°C, 450°C and 600°C.
  • Table 1 also shows the case (2) where Mg and Li were co-doped and the case (4) where Li, F and Mg were co-doped.
  • the Mg was prepared by radiating the microwave level of electromagnetic waves to a corresponding molecular gas or by bringing a corresponding elemental cell into an atomic form under a high temperature.
  • an additional component is only one elemental cell.
  • each of the result of co-doping Li and Mg (2), the result of co-doping Li and F (3), and the result of co-doping Li, F and Mg (4) exhibits a hole concentration having larger digits by three or more.
  • each of the results (2) to (4) exhibits a hole mobility (cm2/V ⁇ g) having larger digits by two or more
  • the resistivity ( ⁇ cm) in inverse proportion to the product of the hole concentration and hole mobility has reduced digits by five or more as compared to the case of singly doping, and goes down to less than 10 ⁇ ⁇ cm when the substrate temperature is 400°C or more.
  • a p-type single-crystal ZnO thin film could be obtained with a high hole concentration of 8 x 10 18 (number/cm 3 ).
  • a p-type single-crystal ZnO thin film having a low resistivity of 10 ⁇ ⁇ cm could be obtained.
  • Fig. 2 shows the configuration of two acceptors and one donor in a ZnO crystal, which is determined by use of the first-principles band structure calculation method. As can be seen in Fig. 2, it has been verified that the crystallographic configuration of Li was stabilized by adding Li as an acceptor and F as a donor in the ZnO crystal, and thereby Li could be doped stably in a high concentration. Mg of the second group element is located substantially independently of Li and F to stabilize oxygen.
  • ZnO of the present invention is a novel low-resistivity p-type single-crystal ZnO which has not been achieved, and this single crystal ZnO has a innovative broader range of applications. Further, the method of the present invention makes it possible to obtain the low-resistivity p-type single-crystal ZnO readily.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Physical Deposition Of Substances That Are Components Of Semiconductor Devices (AREA)
EP00942475A 1999-08-13 2000-07-04 P-typ zinkoxid-einkristall mit niedrigem widerstand und herstellungsverfahren dafür Expired - Lifetime EP1215310B1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP22950499A JP4126332B2 (ja) 1999-08-13 1999-08-13 低抵抗ｐ型単結晶酸化亜鉛およびその製造方法
JP22950499 1999-08-13
PCT/JP2000/004452 WO2001012884A1 (fr) 1999-08-13 2000-07-04 OXYDE DE ZINC MONOCRISTALLIN DE TYPE p PRESENTANT UNE FAIBLE RESISTIVITE ET SON PROCEDE DE PREPARATION

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EP1215310A1 true EP1215310A1 (de) 2002-06-19
EP1215310A4 EP1215310A4 (de) 2003-05-02
EP1215310B1 EP1215310B1 (de) 2007-12-19

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US (1) US6896731B1 (de)
EP (1) EP1215310B1 (de)
JP (1) JP4126332B2 (de)
KR (1) KR100494376B1 (de)
DE (1) DE60037526T2 (de)
TW (1) TW499511B (de)
WO (1) WO2001012884A1 (de)

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WO2004105097A2 (en) * 2003-05-20 2004-12-02 Robert Ii Burgener Fabrication of p-type group ii-vi semiconductors
WO2006009781A2 (en) * 2004-06-17 2006-01-26 On International, Inc. Dynamic p-n junction growth
EP1630218A1 (de) * 2003-04-30 2006-03-01 National Institute for Materials Science Zinkoxid-leuchtstoff, verfahren zu seiner herstellung sowie lichtemittierende vorrichtung
US7172813B2 (en) 2003-05-20 2007-02-06 Burgener Ii Robert H Zinc oxide crystal growth substrate
US20110114937A1 (en) * 2007-08-08 2011-05-19 Rohm Co., Ltd. p-TYPE MgZnO-BASED THIN FILM AND SEMICONDUCTOR LIGHT EMITTING DEVICE
US8137458B2 (en) 2005-08-09 2012-03-20 Stanley Electric Co., Ltd. Epitaxial growth of ZnO with controlled atmosphere

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US6887736B2 (en) * 2002-06-24 2005-05-03 Cermet, Inc. Method of forming a p-type group II-VI semiconductor crystal layer on a substrate
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JP4210748B2 (ja) * 2003-08-27 2009-01-21 独立行政法人物質・材料研究機構 酸化亜鉛基積層構造体
JP4386747B2 (ja) 2004-01-28 2009-12-16 三洋電機株式会社 ｐ型ＺｎＯ半導体膜及びその製造方法
US20070111372A1 (en) * 2004-07-20 2007-05-17 Cermet, Inc. Methods of forming a p-type group ii-vi semiconductor crystal layer on a substrate
JP4677796B2 (ja) * 2005-02-21 2011-04-27 東ソー株式会社 酸化亜鉛単結晶の製造方法
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JP5360789B2 (ja) 2006-07-06 2013-12-04 独立行政法人産業技術総合研究所 ｐ型酸化亜鉛薄膜及びその作製方法
KR100958137B1 (ko) 2008-02-18 2010-05-18 부산대학교 산학협력단 Ｌｉ과 Ⅶ족 불순물을 동시 도핑한 ｐ－형 ＺｎＯ반도체
TW200949004A (en) * 2008-04-25 2009-12-01 Lumenz Inc Metalorganic chemical vapor deposition of zinc oxide
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US7829376B1 (en) 2010-04-07 2010-11-09 Lumenz, Inc. Methods of forming zinc oxide based II-VI compound semiconductor layers with shallow acceptor conductivities
US8722456B2 (en) * 2010-09-25 2014-05-13 Hangzhou Bluelight Opto-electronic Material Co., Ltd. Method for preparing p-type ZnO-based material
EP2787547A4 (de) * 2011-11-28 2015-07-08 Oceans King Lighting Science Polymere solarzelle und verfahren zu ihrer herstellung
JP6092586B2 (ja) * 2012-02-28 2017-03-08 スタンレー電気株式会社 ＺｎＯ系半導体層とその製造方法、及びＺｎＯ系半導体発光素子の製造方法
US9064790B2 (en) 2012-07-27 2015-06-23 Stanley Electric Co., Ltd. Method for producing p-type ZnO based compound semiconductor layer, method for producing ZnO based compound semiconductor element, p-type ZnO based compound semiconductor single crystal layer, ZnO based compound semiconductor element, and n-type ZnO based compound semiconductor laminate structure
JP6017243B2 (ja) * 2012-09-26 2016-10-26 スタンレー電気株式会社 ＺｎＯ系半導体素子、及び、ＺｎＯ系半導体素子の製造方法
JP6100591B2 (ja) * 2013-04-16 2017-03-22 スタンレー電気株式会社 ｐ型ＺｎＯ系半導体層の製造方法、ＺｎＯ系半導体素子の製造方法、及び、ｎ型ＺｎＯ系半導体積層構造
JP6100590B2 (ja) * 2013-04-16 2017-03-22 スタンレー電気株式会社 ｐ型ＺｎＯ系半導体層の製造方法、ＺｎＯ系半導体素子の製造方法、及び、ｎ型ＺｎＯ系半導体積層構造
CN106248736A (zh) * 2016-07-14 2016-12-21 上海纳米技术及应用国家工程研究中心有限公司 乙醇敏感的Co掺杂的分级多孔结构ZnO微球及制备和应用

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RYU Y R ET AL: "Synthesis of p-type ZnO films" JOURNAL OF CRYSTAL GROWTH, JULY 2000, ELSEVIER, NETHERLANDS, vol. 216, no. 1-4, pages 330-334, XP004206254 ISSN: 0022-0248 *
See also references of WO0112884A1 *

Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1630218A1 (de) * 2003-04-30 2006-03-01 National Institute for Materials Science Zinkoxid-leuchtstoff, verfahren zu seiner herstellung sowie lichtemittierende vorrichtung
EP1630218A4 (de) * 2003-04-30 2009-04-29 Nat Inst For Materials Science Zinkoxid-leuchtstoff, verfahren zu seiner herstellung sowie lichtemittierende vorrichtung
US7141489B2 (en) * 2003-05-20 2006-11-28 Burgener Ii Robert H Fabrication of p-type group II-VI semiconductors
WO2004105097A3 (en) * 2003-05-20 2005-06-16 Robert Ii Burgener Fabrication of p-type group ii-vi semiconductors
WO2004105098A3 (en) * 2003-05-20 2005-04-14 Robert H Ii Burgener P-type group ii-vi semiconductor compounds
WO2004105098A2 (en) * 2003-05-20 2004-12-02 Burgener Robert H Ii P-type group ii-vi semiconductor compounds
US7161173B2 (en) * 2003-05-20 2007-01-09 Burgener Ii Robert H P-type group II-VI semiconductor compounds
US7172813B2 (en) 2003-05-20 2007-02-06 Burgener Ii Robert H Zinc oxide crystal growth substrate
US7473925B2 (en) 2003-05-20 2009-01-06 On International, Inc. P-type group II-VI semiconductor compounds
WO2004105097A2 (en) * 2003-05-20 2004-12-02 Robert Ii Burgener Fabrication of p-type group ii-vi semiconductors
WO2006009781A2 (en) * 2004-06-17 2006-01-26 On International, Inc. Dynamic p-n junction growth
WO2006009781A3 (en) * 2004-06-17 2008-10-23 On International Inc Dynamic p-n junction growth
US8137458B2 (en) 2005-08-09 2012-03-20 Stanley Electric Co., Ltd. Epitaxial growth of ZnO with controlled atmosphere
US20110114937A1 (en) * 2007-08-08 2011-05-19 Rohm Co., Ltd. p-TYPE MgZnO-BASED THIN FILM AND SEMICONDUCTOR LIGHT EMITTING DEVICE
US8410478B2 (en) * 2007-08-08 2013-04-02 Rohm Co., Ltd. p-Type MgZnO-based thin film and semiconductor light emitting device

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EP1215310B1 (de) 2007-12-19
DE60037526D1 (de) 2008-01-31
JP2001048698A (ja) 2001-02-20
TW499511B (en) 2002-08-21
KR100494376B1 (ko) 2005-06-10
US6896731B1 (en) 2005-05-24
DE60037526T2 (de) 2008-10-23
EP1215310A4 (de) 2003-05-02
WO2001012884A1 (fr) 2001-02-22
KR20020034174A (ko) 2002-05-08

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